CN103374666A - Preparation method of aluminum boron intermediate alloy - Google Patents

Preparation method of aluminum boron intermediate alloy Download PDF

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Publication number
CN103374666A
CN103374666A CN2012101159139A CN201210115913A CN103374666A CN 103374666 A CN103374666 A CN 103374666A CN 2012101159139 A CN2012101159139 A CN 2012101159139A CN 201210115913 A CN201210115913 A CN 201210115913A CN 103374666 A CN103374666 A CN 103374666A
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CN
China
Prior art keywords
aluminium
melt
master alloy
boron
aluminum
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CN2012101159139A
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Chinese (zh)
Inventor
赵九洲
赵洪生
王青亮
王云利
栗争光
沈利
刘金龙
翟宝晨
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Baotou Aluminium Co ltd
Institute of Metal Research of CAS
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Baotou Aluminium Co ltd
Institute of Metal Research of CAS
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Priority to CN2012101159139A priority Critical patent/CN103374666A/en
Publication of CN103374666A publication Critical patent/CN103374666A/en
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Abstract

The invention discloses a preparation method of an aluminum boron intermediate alloy. According to the method, an aluminum boron intermediate alloy melt is obtained through the chemical reaction of potassium fluoborate and aluminum melt in a vortex salting way. The method concretely comprises the steps of putting an industrial pure aluminium ingot into a crucible to be heated and molten; adding a covering agent on the surface of the melt, wherein the covering agent accounts for 0.5-5% of the weight of the aluminum melt and comprises the components of KAlF4 and Na3AlF6 in the molar ratio of (3-9):1; controlling the temperature of the aluminum melt at 700-850 DEG C, stirring the melt by using a graphite agitator with spirals and forming a vortex; and adding the potassium fluoborate accounting for 40-45% of the weight of the aluminum melt into the center of the vortex, stopping stirring after completing the salting, pouring out villiaumite at the surface layer after holding the temperature for some time, pouring out the melt after fully stirring the intermediate alloy melt, thus obtaining the aluminum boron intermediate alloy. The method has the advantages that the boron recovery rate is high (can be up to above 80%) and AlB2 particles are distributed and dispersed in an aluminum substrate.

Description

A kind of preparation method of aluminium boron master alloy
Technical field
The invention belongs to the technical field of non-ferrous metal, be specifically related to a kind of preparation method of aluminium boron master alloy.
Background technology
At present, the preparation method that aluminium boron master alloy adopts usually is that potassium fluoborate is complete or gradation joins in aluminium melt surface or the molten aluminium, stirs to promote reaction to carry out in the reaction process.Adopt above technique, the volatile decomposition because potassium fluoborate is heated causes the boron rate of recovery lower, generally is lower than 80%, and production cost is high; And in the reaction process, the sheet AlB that from melt, separates out 2Coalescence easily occurs because interfacial tension drives in particle, and forms the cluster tissue, and this will cause bad impact to purifying and the thinning effect of aluminium boron master alloy.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of preparation method that the higher boron rate of recovery (>80%), boride particle disperse are distributed in a kind of aluminium boron master alloy in the aluminum substrate that has is provided.The method can reduce the master alloy production cost, better meets the demand of conductive aluminum production and aluminum grain refinement.
For achieving the above object, technical scheme of the present invention is:
A kind of preparation method of aluminium boron master alloy, the method makes potassium fluoborate (particulate state technical pure potassium fluoborate) and molten aluminium carry out chemical reaction by whirlpool salt adding mode, to obtain aluminium boron intermediate alloy melt; Described whirlpool salt adding mode step is as follows:
1) commercial-purity aluminium is put into the crucible heat fused and formed molten aluminium;
2) add the insulating covering agent that accounts for molten aluminium weight 0.5-5% to aluminium melt surface; Described insulating covering agent is ptfe aluminum potassium (KAlF 4) and sodium aluminum fluoride (Na 3AlF 6) with (3-9): 1 molar ratio mixes;
3) use the graphite whisker with spiral that molten aluminium is stirred, draw whirlpool after, add at the uniform velocity continuously the potassium fluoborate that accounts for molten aluminium weight 40-45% to the whirlpool center; Wherein, agitator speed 600-700r/min, the time length that adds potassium fluoborate is 15-30 minute;
4) salt adding is complete, stops to stir, and after behind the insulation 20min top layer villiaumite being poured out, namely obtains intermediate alloy melt, waters out after it is fully stirred, and obtains aluminium boron master alloy.
Described graphite whisker with spiral, comprise agitator arm and screw mixing head, described stirring-head spiral external diameter is 1 with the ratio of crucible internal diameter: (2-4), the molten aluminium depth ratio is 1 in spiral height and the crucible: (1.5-4), lead angle is 10-30 °, and spiral internal diameter is 1 with the external diameter ratio: (1.2-3).
Control the molten aluminium temperature between 700-850 ℃ by the power of regulating medium-frequency induction furnace in the above-mentioned reaction process.
The present invention has following beneficial effect:
1, the present invention adopts the graphite whisker with spiral that molten aluminium is stirred, because the effect of pressure difference, the potassium fluoborate particle is inhaled in the molten aluminium, at molten aluminium inside and reactive aluminum, can stop the potassium fluoborate volatilization, improved the rate of recovery of boron, the shearing force of melt being carried out the mechanical stirring generation can stop AlB 2The formation of particle clusters improves AlB 2The disperse degree of particle.
2, the aluminium boron master alloy of the present invention's preparation has the higher boron rate of recovery (>80%), the boride particle disperse is distributed in the aluminum substrate, and the method can reduce the master alloy production cost, better meets the demand of conductive aluminum production and aluminum grain refinement.
Description of drawings
Fig. 1 is reaction unit synoptic diagram of the present invention; Wherein: 1-crucible, 2-graphite whisker, 3-salt adding device, 21-agitator arm, 22-screw mixing head.
To be the embodiment of the invention 1 boron-containing quantity be the aluminium boron master alloy sample microtexture of~3wt% to Fig. 2; White is aluminum substrate among the figure, and grizzled particle is AlB 2, black is residual salt slag inclusion mutually.
To be the embodiment of the invention 2 boron-containing quantitys be the aluminium boron master alloy sample microtexture of~3wt% to Fig. 3.White is aluminum substrate among the figure, and grizzled particle is AlB 2, black is residual salt slag inclusion mutually.
To be the embodiment of the invention 3 boron-containing quantitys be the aluminium boron master alloy sample microtexture of~3wt% to Fig. 4.White is aluminum substrate among the figure, and grizzled particle is AlB 2, black is residual salt slag inclusion mutually.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Equipment therefor of the present invention as shown in Figure 1, commercial-purity aluminium is put into plumbago crucible 1, uses the 2 pairs of molten aluminiums of graphite whisker with spiral to stir, and adds the potassium fluoborate particle to the vortex core by the salt adding device.Wherein said graphite whisker 2 with spiral comprises agitator arm 21 and screw mixing head 22, described stirring-head 22 its spiral external diameters are 1 with the ratio of plumbago crucible 1 internal diameter: (2-4), spiral height and plumbago crucible 1 interior molten aluminium depth ratio are 1: (1.5-4), lead angle is 10-30 °, and spiral internal diameter is 1 with the external diameter ratio: (1.2-3).
Embodiment 1
Get 1000g technical pure aluminium ingot, 420g particulate state potassium fluoborate, 50g composition are mol ratio KAlF 4: Na 3AlF 6=9: 1 insulating covering agent adopts graphite whisker, and its spiral external diameter of the stirring-head of agitator is 1: 2.5 with crucible 1 internal diameter ratio, and spiral height and molten aluminium depth ratio are 1: 2.5, and lead angle is 17.5 °, and spiral internal diameter is 1: 2 with the external diameter ratio.
Operating process is as follows: commercial-purity aluminium is put into plumbago crucible heat (operating frequency is 1800Hz) with medium-frequency induction furnace, melt backward bath surface and be sprinkled into insulating covering agent, when being warming up to 700 ℃, use is carried out mechanical stirring with the graphite whisker of spiral to molten aluminium, agitator speed is 600-700r/min, makes melt produce whirlpool; Add at the uniform velocity continuously the potassium fluoborate particle to the vortex core, regulate medium-frequency induction furnace power, make that melt temperature remains between 700-750 ℃ in the reaction process, salt adding (salt the refers to potassium fluoborate) time is 20min; Salt adding is complete, stops to stir, and behind the insulation 20min fused salt is poured out; The abundant stir about of melt is poured into after 1 minute in the swage that diameter is Φ 80mm, be frozen into aluminium boron master alloy.
Metallurgical analysis shows, AlB 2Particle dispersion is distributed in the aluminum substrate, sees Fig. 2.Chemical analysis shows that boron content is 3.2wt% in the master alloy, and the boron rate of recovery is 84.7%.
Embodiment 2
Starting material comprise: 1050g technical pure aluminium ingot, and 450g particulate state analytical pure potassium fluoborate, the 40g composition is mol ratio KAlF 4: Na 3AlF 6=6: 1 insulating covering agent adopts graphite whisker, and stirring-head spiral external diameter is 1: 3 with crucible 1 internal diameter ratio, and spiral height and molten aluminium aspect ratio are 1: 2.2, and lead angle is 17.5 °, and spiral internal diameter is 1: 2 with the external diameter ratio.
Operating process is as follows: commercial-purity aluminium is put into plumbago crucible by medium-frequency induction furnace heating (operating frequency is 1800Hz), melt backward bath surface and be sprinkled into insulating covering agent, when being warming up to 750 ℃, use is carried out mechanical stirring with the graphite whisker of spiral to molten aluminium, agitator speed is 600-700r/min, makes melt produce whirlpool; Add at the uniform velocity continuously the potassium fluoborate particle to the vortex core, regulate medium-frequency induction furnace power, make that melt temperature remains between 750-800 ℃ in the reaction process, the salt adding time is 18min; Salt adding is complete, stops to stir, and behind the insulation 20min fused salt is poured out; The abundant stir about of melt is poured into after 1 minute in the swage that diameter is Φ 80mm, be frozen into aluminium boron master alloy.
Metallurgical analysis shows, AlB 2Particle dispersion is distributed in the aluminum substrate, sees Fig. 3.Chemical analysis shows that boron content is 3.3wt% in the master alloy, and the boron rate of recovery is 85.5%.
Embodiment 3
Starting material comprise: 1200g technical pure aluminium ingot, and 500g particulate state analytical pure potassium fluoborate, the 60g composition is mol ratio KAlF 4: Na 3AlF 6=4: 1 insulating covering agent adopts graphite whisker, and stirring-head spiral external diameter is 1: 3 with crucible 1 internal diameter ratio, and spiral height and molten aluminium aspect ratio are 1: 3, and lead angle is 12 °, and spiral internal diameter is 1: 2.5 with the external diameter ratio.
Operating process is as follows: commercial-purity aluminium is put into plumbago crucible by medium-frequency induction furnace heating (operating frequency is 1800Hz), melt backward bath surface and be sprinkled into insulating covering agent, when being warming up to 800 ℃, use is carried out mechanical stirring with the graphite whisker of spiral to molten aluminium, agitator speed is 600-700r/min, makes melt produce whirlpool; Add at the uniform velocity continuously the potassium fluoborate particle to the vortex core, regulate medium-frequency induction furnace power, make that melt temperature remains between 800-850 ℃ in the reaction process, the salt adding time is 15min; Salt adding is complete, stops to stir, and behind the insulation 20min fused salt is poured out; The abundant stir about of melt is poured into after 1 minute in the swage that diameter is Φ 80mm, be frozen into aluminium boron master alloy.
Metallurgical analysis shows, AlB 2Particle dispersion is distributed in the aluminum substrate, sees Fig. 4.Chemical analysis shows that boron content is 3.1wt% in the master alloy, and the boron rate of recovery is 82.4%.

Claims (6)

1. the preparation method of an aluminium boron master alloy, it is characterized in that: the method makes potassium fluoborate and molten aluminium carry out chemical reaction by whirlpool salt adding mode, to obtain aluminium boron intermediate alloy melt; Described whirlpool salt adding mode step is as follows:
1) aluminium is put into the crucible heat fused and formed molten aluminium;
2) add the insulating covering agent that accounts for molten aluminium weight 0.5-5% to aluminium melt surface;
3) use the graphite whisker with spiral that molten aluminium is stirred, draw whirlpool after, add at the uniform velocity continuously the potassium fluoborate that accounts for molten aluminium weight 40-45% to the whirlpool center;
4) salt adding is complete, stops to stir, and after behind the insulation 20min top layer villiaumite being poured out, namely obtains intermediate alloy melt, waters out after it is stirred, and obtains aluminium boron master alloy.
2. the preparation method of aluminium boron master alloy according to claim 1, it is characterized in that: described graphite whisker with spiral comprises agitator arm and screw mixing head; Described stirring-head spiral external diameter is 1 with the ratio of crucible internal diameter: (2-4), the molten aluminium depth ratio is 1 in spiral height and the crucible: (1.5-4), lead angle is 10-30 °, and spiral internal diameter is 1 with the external diameter ratio: (1.2-3).
3. the preparation method of aluminium boron master alloy according to claim 1 is characterized in that: control the molten aluminium temperature in the reaction process between 700-850 ℃.
4. the preparation method of aluminium boron master alloy according to claim 1 is characterized in that: described insulating covering agent is ptfe aluminum potassium and sodium aluminum fluoride with (3-9): 1 molar ratio mixes.
5. the preparation method of aluminium boron master alloy according to claim 1 is characterized in that: step 3) middle agitator speed 600-700r/min, the time length that adds potassium fluoborate is 15-30 minute.
6. the preparation method of aluminium boron master alloy according to claim 1, it is characterized in that: described aluminium is the technical pure aluminium ingot, described potassium fluoborate is particulate state technical pure potassium fluoborate.
CN2012101159139A 2012-04-19 2012-04-19 Preparation method of aluminum boron intermediate alloy Pending CN103374666A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107916342A (en) * 2017-11-29 2018-04-17 河北晶宝新金属有限公司 A kind of production technology of aluminum-boron alloy bar
CN108220641A (en) * 2017-12-15 2018-06-29 南通昂申金属材料有限公司 A kind of preparation method of aluminium boron intermediate alloy
CN109355520A (en) * 2018-11-27 2019-02-19 中国科学院金属研究所 A kind of Al-Ti-C-B intermediate alloy and preparation method thereof

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CN101994027A (en) * 2010-12-10 2011-03-30 株洲冶炼集团股份有限公司 Direct production method for lead calcium rare earth alloy

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US5415708A (en) * 1993-06-02 1995-05-16 Kballoys, Inc. Aluminum base alloy and method for preparing same
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CN201347461Y (en) * 2009-01-07 2009-11-18 永城科源电子铝箔有限公司 Movable graphite whisker
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107916342A (en) * 2017-11-29 2018-04-17 河北晶宝新金属有限公司 A kind of production technology of aluminum-boron alloy bar
CN108220641A (en) * 2017-12-15 2018-06-29 南通昂申金属材料有限公司 A kind of preparation method of aluminium boron intermediate alloy
CN109355520A (en) * 2018-11-27 2019-02-19 中国科学院金属研究所 A kind of Al-Ti-C-B intermediate alloy and preparation method thereof
CN109355520B (en) * 2018-11-27 2020-10-09 中国科学院金属研究所 Al-Ti-C-B intermediate alloy and preparation method thereof

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